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  • Optimization and application of headspace-solid-phase micro-extraction coupled with gas chromatography-mass spectrometry for the determination of volatile compounds in cherry wines.

Optimization and application of headspace-solid-phase micro-extraction coupled with gas chromatography-mass spectrometry for the determination of volatile compounds in cherry wines.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2014-12-30)
Zuobing Xiao, Xuan Zhou, Yunwei Niu, Dan Yu, Jiancai Zhu, Guangyong Zhu
ABSTRACT

A simple, rapid and solvent-free multi-residue method has been developed and applied to confirm and quantify a series of volatile compounds in five cherry wines by gas chromatography coupled with mass spectrometry (GC-MS). Four parameters (e.g., coating material of fiber, temperature and time of extraction, and addition of sodium chloride in the solution) of headspace solid-phase micro-extraction (HS-SPME) were optimized, resulting in the best extraction condition including 50/30 μm DVB/CAR/PDMS fiber, 45 min and 50 °C of SPME, and 2g of sodium chloride addition in the wine during the extraction. The SPME had LODs and LOQs ranging from 0.03 to 7.27 μg L(-1) and 0.10 to 24.24 μg L(-1) for analytic compounds, respectively. Repeatability and reproducibility values were all below 19.8%, with mean values of 12.7% and 10.5%, respectively. Regression coefficients (R(2)) of detective linearity of the standard curves was higher than 0.9852. Moreover, relative recoveries of analytical targets were achieved in a range of 60.7-125.6% with good relative standard deviation values (≤20.6%). In addition, a principal component analysis (PCA) was used to analyze the aroma profiles of the wines, which indicated that five samples were distinctly divided into two groups based on their different geographical origins and volatile compounds.

MATERIALS
Product Number
Brand
Product Description

Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm(PEG, metal alloy fiber, for use with manual holder
Supelco
SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm(PEG, for use with autosampler
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
Sigma-Aldrich
Sodium chloride, tested according to Ph. Eur.
Sigma-Aldrich
Sodium chloride, BioUltra, for molecular biology, ≥99.5% (AT)
Supelco
Acetic acid, analytical standard
Sigma-Aldrich
Sodium chloride solution, BioUltra, for molecular biology, ~5 M in H2O
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 1 cm
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, for use with autosampler, needle size 23 ga, metal alloy fiber
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm
Sigma-Aldrich
Sodium hydroxide, BioUltra, for luminescence, ≥98.0% (T), pellets
Sigma-Aldrich
Sodium hydroxide solution, BioUltra, for molecular biology, 10 M in H2O
Sigma-Aldrich
Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
Supelco
Sodium hydroxide solution, 49-51% in water, eluent for IC
Supelco
Sodium chloride, reference material for titrimetry, certified by BAM, >99.5%
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
Sigma-Aldrich
Acetic acid, natural, ≥99.5%, FG
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Hexamethyldisiloxane, viscosity 0.65 cSt (25 °C)
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Divinylbenzene, technical grade, 80%
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Sodium chloride, 99.999% trace metals basis
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Ethyl lactate, natural, ≥98%, FCC, FG
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1-Butanol, anhydrous, 99.8%
Sigma-Aldrich
Divinylbenzene, technical grade, 55%
Sigma-Aldrich
2-Octanol, ≥97%, FG
Sigma-Aldrich
Ethanol, anhydrous, denatured
Sigma-Aldrich
Sodium chloride-35Cl, 99 atom % 35Cl
Sigma-Aldrich
Sodium chloride, random crystals, optical grade, 99.9% trace metals basis
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler